Production of hydrogen sodium sulphide



My 23, @929 H, P, BA sE -r 22370 PRODUCTION OF HYDROGEN SODIUM SULPHIDE Filed Oct. 9/1925 AND GOKE

Nah 6 hi iqnsa rr 61cm H1341 cool out of contact with the air.- I

The mixture of calcium compounds and Patented .luly 23, 1929.

,UNITED STATES,

' many nassn'rr, :OFZCYNTHIANA, KENTUCKY.

Q raonucrron ornrnRoGEN sonfum: sunrmnn Application filed October 9, 1925. Serial No. 61,594.

This invention relates to the production of hydrogen sodium sulphide from calcium sulfate in a process which is to a considerable extentcyclic, in that several of the products 5 producedtherein are adapted for use in the treatment'of additional material at different stages of the process thereby effecting a substantial economy in the production of the hydrogen sodium sulphide. I The singlefigure of the drawing is a flow sheet illustrating my invention.

In thepractice of my process in itspre ferred' form, I first heat to a reducing tem perature a; mixture of pulverized calcium.

' sulfate'with about 25 per cent by weight of carbonaceous matter preferably-a mixture of owdered coal and coke, the coalfand coke eing presentin the proportions 0154 parts by weight of the former to '3. parts by weight of the'latter. The mixture ispreferably sub-- jected to a temperature of'from about 1100 to 1600 F., in a batch furnace, such for ex ample, as the Brockner furnace, or in a rotary tube furnace of ordinary construction; The mixtureis heated in a reducing atmosphere and in thetreatment of:2000 pounds of calcium sulfate, the reducin operation at the preferred temperature in icated above ordinarily requires about one hour or longer.

Theproduct of the reaction is coke, which may be used in thetreatment of additional calcium sulfate, and a mixture of calcium compounds consisting entirely or almost entirely of calcium sulphide, calcium sulfite and pounds and cokeis preferably allowed to coke is then-placed ina closed chamber adapted .to withstand considerable internal pressure and to the mixture is added a solusulfate of any desired preferably of a strength below saturation, the amount of sodium sulfate used being less than in molecular proportions with respect to the calcium sulphide present. The mixture is then heated under a tion of sodium strength althoug pressure which is essentially in excess of atmospheric pressure and I prefer to heat the mixture under a pressure of about 25 to 30 pounds in excess of atmospheric pressure, a temperature of around 236 to 250 F. being well suited to the reaction. The treatment must be conducted at superatmo'spheric pressure buts'orne measure of success is obtainresulting mixture and the. solution after' calcium o'xid. The mixtureofcalcium com ableif the pressure is only slightly above atmospheric pressure as, for example, at 5 pounds superatmospheric pressure although prefer to use higher pressures.

As a result of this treatment, sodium sulphide and calcium sulfateresult from the reaction of sodium sulfate and calcium sulphide.

The sodium sulphide is leached out ofthebeing filtered contains sodium sulphide sufiiciently .pu're for the production of hydrogen sod um sulphide adapted for use in the artificial -silk industry. 7 The coke and calcium sulfate remaining '0 after the leaching operation may be used with additional calcium sulfate and coal in the first staged the 'process' The filtered solution of sodium sulphide is divided into two approximately equal parts and to oneyof the parts is added sulfuric acid or its equivalent such as .sodium hydrogen sulfate to react with the sodium sulphide to producehydrogen sulphide and sodium sulfate. The hydrogen sulphide is conducted mto the other part of the filtered sodium sulphidesolution producing hydrogen sodium.

sulphide adapted without further treatment for use in the artificialsilk and other chemical industries. The remaining sodium sulfate is used in the treatment of additional quantities of calcium sulphide in an intermediate step of my process.

My process produces hydrogen sodium sulphide of a highdegree of .purity and at a low cost of production, the utilization of products of the ste s ofthe process in the treatment of additiona quantities of material at earlier stages of the process serving to efiect sub stantial economies.

While I have described in detail the preferred practice of my process, it is to be understood that the procedure ma: be variously modifiedand that other suitable reduc ing a 'paratus than those herein referred to may. e employed without departing from the spirit of my invention or the scope of the subjoined claims.

Having thus described. my invention, I claim: 1

'1. The process of making hydrogenj sodium sulphide comprising heating calcium sulfate to a reducing temperature with carbonaceous matter to produce calcium sulphide, calcium sulfite and calcium oxid, heat- 110 ing-such calcium salts with a solution of soparts, addin sulfuric acid to one of the parts dium sulfate, such sodium sulfate being present in less than molecular proportions with- .to produce ydrogensulphide and sodium sulfate, conducting the hydrogen sulphide respect to the calcium sulphide present, at intQ theother part to produce hydrogen sosuperatmospheric pressure to produce sodium sulphide, leaching the product of the reaction, dividing the solution resulting from the leaching operation into two parts, acting upon one of the parts with an acid adapted to transform sodium sulphide into hydrogen sulphide and conducting the hydrogen sulphide produced into the other part of the solution resulting from the leaching opera- .tion to produce hydrogen sodium sulphide.

the leaching operation into two parts, adding sulfuric acid to one of the parts to produce hydrogen sulphide and sodium sulfate, and conducting the hydrogen sulphide into the other part to produce hydrogen sodium sulphide.

3. The process of making hydrogen sodium sulphide comprising heating a mixture of calcium sulfate, coal and coke to a reducing temperature to produce coke and a mix? ture of calcium compounds comprising calcium suphide, calcium sulfite and calcium oxid, heating the products of the reducing reaction at superatniospheric pressure with a solution of sodium sulfate, the sodium sulfate being present in less than molecular proportions with respect to the calcium sulphide present, to produce sodium sulphide and calcium sulfate, leaching the roduct of the reaction, separating the solution resulting from the leaching operation into two dium sulphide, and employing the mixture of coke and calcium sulfate resulting from the second step of the process in the first step of the process.

4. The process of making hydrogen sodium sulphide comprising heating a mixture of calcium sulfate, coal and coke to a reducmg temperature to produce coke and a mixture of calcium compounds comprising calcium sulphide, calcium sulfite and calcium oxid, heating the products of the reducing reaction at superat'mospheric pressure with a solution of sodium sulfate, the sodium sulfate being present in less than molecular proportions with respect'to thecalcium sulphide present, to produce sodium sulphide and calcium sulfate, leaching the product of the reaction, separating the solution resultmg from-the leaching operation into two parts, adding sulfuric acid toone of the parts to produce hydrogen sulphide and sodium sulfate, conducting-the hydrogen sulphide into the other part to produce hydrogen sodium sulphide, employing the mixture of coke and calcium sulfate resulting from the second step of the process in the first step of the process, and employing the sodium sulfate produced in the reaction of sulfuric acid on the sodium sulphide in the treatment of additional calcium sulphide in the second step of the process.

5. In the herein described process, the steps of heating a mixture of calcium sulfate and carbonaceous matter to a reducing temperature to produce coke and calcium compounds comprising calcium sulphide, calciumsulfite and calcium oxid, adding sodium sulfate. in solution in less than molecular proportions with respect to the calcium sulphide present, heating the mixture at super-atmospheric pressure, leaching the product, and employing theresidue from the leaching operation in the first step of the process.

' In testimony whereof I afiix m signature. HARRY P. B SSETT. 

